N-bromobutanimide → 5-bromo-2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone

HRID 2400099

反応式

HRID 2400099 の反応式
[C:1]1([C:7]2[NH:12][C:11](=[O:13])[CH:10]=[C:9]([C:14]([F:17])([F:16])[F:15])[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:18]N1C(=O)CCC1=O>C(O)(=O)C>[Br:18][C:10]1[C:11](=[O:13])[NH:12][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8][C:9]=1[C:14]([F:16])([F:17])[F:15]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 1354100074-Hydroxy-2-phenyl-6-(trifluoromethyl)pyrimidine

生成物 1

HCID 1358375345-bromo-2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone収率 83.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 1.0 g (3.94 mmol) of 2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone and 20 mL of glacial acetic acid was added 1.0 g (5.6 mmol) N-bromosuccinimide and the mixture was left to stir at room temperature for 16 h. The reaction was poured onto ice water and vacuum filtered, washing well with water. The crude product was recrystallized from ethyl acetate to yield 1.05 g (83.5%) of 5-bromo-2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone, as a white solid. 1H-NMR (d6DMSO)δ7.6 (3H, m); 8.15 (2H, m).

後処理

  1. waitthe mixture was left
  2. additionThe reaction was poured onto ice water and vacuum
  3. filtrationfiltered
  4. washwashing well with water
  5. customThe crude product was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-a2589baa386f4cb68df2e82406942c40
出典データセット
uspto-grants-1995_09
特許番号
US05453414

関連ノート

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